Potassium Carbonate → 4-((4-(3-((6-Chloro-2-naphthyl)sulfonyl)propanoyl)-1-piperazinyl)methyl)-1,3-thiazol-2-amine

HRID 493697

반응식

HRID 493697 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([CH2:15][CH2:16][C:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)=[O:18])(=[O:14])=[O:13])[CH:6]=[CH:5]2.Cl.Cl[CH2:27][C:28]1[N:29]=[C:30]([NH2:33])[S:31][CH:32]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([CH2:15][CH2:16][C:17]([N:19]1[CH2:20][CH2:21][N:22]([CH2:27][C:28]3[N:29]=[C:30]([NH2:33])[S:31][CH:32]=3)[CH2:23][CH2:24]1)=[O:18])(=[O:14])=[O:13])[CH:6]=[CH:5]2

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 732282-Thiazolamine, 4-(chloromethyl)-, hydrochloride (1:1)HCID 231308831-(3-((6-Chloro-2-naphthyl)sulfonyl)propionyl)piperazine

생성물 1

HCID 231309094-((4-(3-((6-Chloro-2-naphthyl)sulfonyl)propanoyl)-1-piperazinyl)methyl)-1,3-thiazol-2-amine수율 71.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (1.5 g) obtained in Example 3a), 4-chloromethyl-1,3-thiazol-2-amine hydrochloride (0.76 g) and potassium carbonate (1.12 g) in acetonitrile (50 mL) was refluxed for 4 hours, and then the solvent was distilled off under reduced pressure. The residue was diluted with potassium carbonate, and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified with a basic silica gel column to give the title compound (1.4 g) as white crystals.

후처리

  1. temperaturewas refluxed for 4 hours
  2. distillationthe solvent was distilled off under reduced pressure
  3. additionThe residue was diluted with potassium carbonate
  4. extractionextracted with chloroform
  5. dry with materialThe extract was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified with a basic silica gel column

출처 및 근거

ORD 기록
ord-88f04dc7c1474d78b2589abb32546252
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534887B2

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